CN111948321A - Method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry - Google Patents
Method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry, belonging to the technical field of rapid analysis and detection. The method comprises the steps of collecting samples, heating and incubating, establishing a classification model by adopting a principal component analysis method, preprocessing data before establishing the model, specifically, filtering the data by a standard deviation option, normalizing by using median standardization, converting logarithmic data, and finally performing principal component analysis after full-range scale processing; the different millet samples are distinguished according to the main component analysis result; the similarity between different varieties of millet can be seen. The invention can carry out trace analysis and two-dimensional separation detection on the millet sample, greatly improves the accuracy of detection of the aroma substances, has higher sensitivity, shortens the detection time and meets the requirements of quick detection and analysis.
Description
Technical Field
The invention belongs to the technical field of rapid analysis and detection, and particularly relates to a method for evaluating aroma components of millets of different varieties based on Gas Chromatography-Ion Mobility spectrometry (GC-IMS).
Background
Millet (Foxtail Millet) belongs to the family poaceae, the genus setaria, the name chestnut, commonly known as Millet, and originates from the yellow river basin of china, and has a history of about 8000 years to date. Millet is widely distributed in China, at present, up to 23 provinces with statistical areas exist, millet is mainly distributed in Shandong, Shanxi, Hebei, Henan, inner Mongolia, Liaoning, Shanxi, Heilongjiang, Gansu and Jilin, and the millet areas of the 10 provinces account for 96.9 percent of the whole country. Wherein, Hebei, Shanxi and inner Mongolia are the main provinces of millet in China, and the yield accounts for 25.3%, 17.9% and 15% of the total yield of millet in China respectively. Millet is rich in nutrition, contains various vitamins, minerals, essential amino acids, unsaturated fatty acids and other nutrient substances necessary for human bodies, and also contains various bioactive substances beneficial to the human bodies, so that millet is often regarded as a dietary supplement for treating type II diabetes, obesity, cardiovascular diseases and the like at present. Due to the growing consumer demand for health foods, it is expected that millets will be consumed more widely in the future. The aroma is an important index influencing the edible quality of millet, and the research on the aroma of millet is mainly developed by technologies such as sensory analysis, gas chromatography-mass spectrometry, electronic nose and the like. Sensory analysis requires professional experimenters, is easily influenced by external factors, and wastes time and labor. The gas chromatography-mass spectrometry technology has the defects of difficult identification of isomers, complex operation, long analysis time, expensive equipment and the like, and is difficult to popularize in China. The electronic nose has the defects of poor detection precision and unqualified components. The traditional flavor research method cannot meet the evaluation effect and efficiency of millet aroma at present, so that a new method for quickly and efficiently evaluating millet aroma components is urgently needed to be explored.
Ion Mobility Spectroscopy (IMS) was first introduced at the end of the 60's 20 th century as a tool technology for detecting trace amounts of gaseous organic compounds at atmospheric pressure. The principle of the IMS technology is that sample steam is converted into ions under atmospheric pressure, enters a drift region through an ion grid gate under the action of a weak electric field, and finally reaches a detector through a drift gas shift region. Compared with other technologies, the gas chromatography and ion mobility spectrometry combined technology (GC-IMS) has higher sensitivity, can perform trace analysis and two-dimensional separation detection on a sample, greatly improves the accuracy of mixture detection, shortens the detection time, and meets the requirements of rapid detection and analysis.
Disclosure of Invention
The invention aims to provide a method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry, which is characterized in that a rapid and efficient quality evaluation method for the aroma components of the millets is established by adopting a gas chromatography-ion mobility spectrometry (GC-IMS) technology, and specifically comprises the following steps:
step 4, extracting characteristic areas of different millet fingerprints by using a comparison method according to the difference of peak intensity signals or colors of characteristic substances in the fingerprints;
and 5, establishing a classification model by adopting a principal component analysis method, and performing orthogonal transformation and dimension reduction on the fragrance substance peak intensity data in all the characteristic regions to finish the distinguishing of different millet samples.
In the step 1, 5g of each collected sample is respectively placed in a 20m L headspace bottle.
The step 2 is to carry out testing by GC-IMS through headspace sampling, and the specific parameters are set as follows: type of column: FS-SE-54-CB-0.5 column (15 m.times.0.53 mm); column temperature: 40 ℃; carrier gas flow: 0-2min,5mL/min, 2-20min,5mL/min-100m L/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 98 deg.C; sample introduction volume: 500 mu L of the solution; analysis time: and 15 min.
Said step 3 collecting retention time, migration rate and relative separationEstablishing a fingerprint spectrum based on the data of the sub-peak intensity, wherein the ordinate is gas phase retention time, the abscissa is ion migration time, the left vertical line is an RIP peak (reaction ion peak, drift time is 8.03ms), and each point on two sides of the RIP peak represents the concentration of one volatile organic compound; the RIP peak is interrupted because the charges carried by the hydrated protons are taken away by the substances with the same gas phase retention time on the right side; and by GCThe qualitative analysis is carried out on the substance by an NIST gas phase retention index database and an IMS migration time database of G.A.S. which are arranged in IMS Library Search software.
Step 4, a comparison method is used, namely, the characteristic regions of different millet fingerprints are extracted according to the difference of peak intensity signals or colors of characteristic substances in the fingerprints; the characteristic region of the millet fingerprint consists of all volatile organic matter signal peaks contained in the sample millet, and each column is an organic matter under the same retention time and drift time, namely the signal peaks of the same substances in different samples.
Step 5, a classification model is established by adopting a principal component analysis method, data needs to be preprocessed before establishing the model, specifically, data is filtered through a standard deviation option, normalization is carried out by utilizing median normalization, then logarithmic data conversion is adopted, and finally principal component analysis is carried out after full-range scale processing; the similarity between different varieties of millets can be seen through the principal component analysis result, and the differentiation of different millet samples is completed.
The invention has the advantages that the gas phase ion mobility spectrometry technology is applied to the analysis of the millet sample for the first time; the method can visually compare the difference between millets of different varieties according to the change of the aroma fingerprint spectrogram of the sample, finish the distinguishing of different millet samples, and simultaneously, can further adopt a chemometrics means to realize the quick and accurate distinguishing of the millets of different varieties. Compared with the prior art, the gas-phase ion mobility spectrometry technology does not need a pretreatment process, and avoids the interference of an external solvent. In addition, the method also has the advantages of low detection limit, short detection time, abundant detection substances, simple and easy analysis operation, high result accuracy and the like, thereby having higher application value.
Drawings
FIG. 1 two-dimensional fingerprint of fragrance substance of Peak Red valley
FIG. 2-4 is a Gallery Plot of fragrance substance peaks selected from gas phase ion mobility spectrograms of different varieties of millet samples;
FIG. 5 principal Components analysis of different varieties of millet samples
Detailed Description
The invention provides a method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry, which adopts a gas chromatography-ion mobility spectrometry (GC-IMS) technology to establish a quick and efficient quality evaluation method for the aroma components of the millets, and specifically comprises the following steps:
step 4, extracting characteristic areas of different millet fingerprints by using a comparison method according to the difference of peak intensity signals or colors of characteristic substances in the fingerprints;
and 5, establishing a classification model by adopting a principal component analysis method, and performing orthogonal transformation and dimension reduction on the fragrance substance peak intensity data in all the characteristic regions to finish the distinguishing of different millet samples. The invention is further described with reference to the following figures and examples.
The embodiment adopts a gas chromatography-ion mobility spectrometry (GC-IMS) technology to establish a quick and efficient quality evaluation method for millet aroma components, and comprises the following specific steps:
1, collecting a sample: weighing 5g samples of Haemangg (FH), ZN21, Chi 6(CG6), Chi 17(CG17), Zhang miscellaneous cereal 10 (ZZ10), Chi 8 (CG8), Yu cereal 18 (YG18), Zhonggu 2 (ZG2), Huangjin cereal (HJ) and Hongmuitou crushing car (HM) and placing the samples in 20m L headspace bottles respectively.
2, the millet is incubated at 95 ℃ for 15 minutes, and is tested by GC-IMS through headspace sample injection, and the specific parameters are set as follows: type of column: FS-SE-54-CB-0.5 column (15 m.times.0.53 mm); column temperature: 40 ℃; carrier gas flow: 0-2min,5mL/min, 2-20min,5mL/min-100m L/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 98 deg.C; sample introduction volume: 500 mu L of the solution; analysis time: and 15 min.
And 3, collecting data of retention time, migration rate and relative ion peak intensity, and establishing a fingerprint spectrum based on the data, wherein the two-dimensional fingerprint spectrum of the aroma substances in the peak red valley is shown in figure 1. In fig. 1, the ordinate is gas phase retention time, the abscissa is ion migration time, and the left vertical line of the graph is RIP peak (reaction ion peak, drift time is 8.03 ms); each point on both sides of the RIP peak represents a volatile organic compound, the white circle represents a low concentration, and the black point in the circle represents a high concentration; the RIP peak is interrupted because the charges carried by the hydrated protons are taken away by the substances with the same gas phase retention time on the right side; (ii) a The numbers next to the circles in fig. 1 indicate different peak materials.
By GCQualitative analysis is carried out on substances by an NIST gas phase retention index database arranged in IMS Library Search software and an IMS migration time database of G.A.S., wherein the qualitative result of the two-dimensional fingerprint spectrum of the fragrant substances of the peak red valley millet is shown in Table 1.
In addition, the millet is incubated at 60 ℃ for 40 minutes by using the GC-MS technology and then injected into an instrument to complete analysis, wherein the GC-MS qualitative result of the fragrance substances of the peak red valley millet is shown in Table 2. Comparing table 1 and table 2, it can be seen that more aroma is obtained by GC-IMS, which on the one hand is more extracted due to increased incubation temperature, and on the other hand shows high sensitivity and low detection limit of GC-IMS to aroma.
And 4, extracting characteristic areas of different millet fingerprints by using a comparison method, namely extracting the characteristic areas of different millet fingerprints according to the difference of peak intensity signals or colors of characteristic substances in the fingerprints. The results are shown in FIG. 2. Each line in fig. 2 is a millet sample, the characteristic region of the millet fingerprint consists of all the volatile organic matter signal peaks contained in the sample, and each column is the signal peak of organic matter (the same substance in different samples) under the same retention time and drift time. The 10 millet samples contained some common volatile components, such as butyl acetate, 2-methyl propanol, valeraldehyde, etc., as can be seen in fig. 2; many volatile components are present in 10 millet samples, but the concentrations differ as follows: 3-methyl butyl acetate, ethyl hexanoate, ethyl 3-methylbutyrate, and the like, as can be seen in FIG. 3; in addition, figure 4 can find that certain volatile substances are present in higher concentrations in some millet samples, such as benzaldehyde in the middle valley No. 2, 1-octen-3-ol in the red valley No. 8, the yu valley No. 18, the middle valley No. 2, and the red shoot breaker.
And 5, establishing a classification model by adopting a principal component analysis method to finish the distinguishing of different millet samples. The method comprises the steps of preprocessing data before modeling, specifically, filtering the data through a standard deviation option, normalizing by using median normalization, converting logarithmic data, and finally performing principal component analysis after full-range scale processing. The similarity between millets of different varieties can be seen through the position distribution of the main component analysis results of millets of various varieties in figure 5, such as: the three samples of ZN17, Chigu 6 CG6 and Chigu 17 CG17 are very close in position, which shows that the similarity is very high from the fragrance perspective; the peak red valley and the middle valley No. 2 are similar to the individual species except that the species is different from most varieties of millet.
TABLE 1 qualitative result of two-dimensional fingerprint of fragrant substances of millet
TABLE 2 qualitative results of millet aroma GC-MS
Claims (6)
1. A method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry is characterized in that a rapid and efficient quality evaluation method for the aroma components of the millets is established by adopting a gas chromatography-ion mobility spectrometry (GC-IMS) technology, and specifically comprises the following steps:
step 1, collecting a sample;
step 2, incubating the millet for 15 minutes at 95 ℃, and testing by GC-IMS through headspace sample injection;
step 3, collecting data of retention time, migration rate and relative ion peak intensity, establishing a fingerprint spectrum based on the data, and simultaneously carrying out qualitative analysis on the aroma substances by adopting an NIST gas phase retention index database built in GC x IMS Library Search software and an IMS migration time database of G.A.S.;
step 4, extracting characteristic areas of different millet fingerprints by using a comparison method according to the difference of peak intensity signals or colors of characteristic substances in the fingerprints;
and 5, establishing a classification model by adopting a principal component analysis method, and performing orthogonal transformation and dimension reduction on the fragrance substance peak intensity data in all the characteristic regions to finish the distinguishing of different millet samples.
2. The method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry as claimed in claim 1, wherein 5g of collected samples are respectively placed in 20mL headspace bottles in step 1.
3. The method for perfuming millet of different varieties based on gas phase ion mobility spectrometry as claimed in claim 1The component evaluation method is characterized in that the step 2 is to test by GC-IMS through headspace sampling, and the specific parameters are set as follows: type of column: FS-SE-54-CB-0.5 column (15 m.times.0.53 mm); column temperature: 40 ℃; carrier gas flow: 0-2min,5mL/min, 2-20min,5mL/min-100 mL/min; drift gas flow rate: 150 mL/min; carrier gas/drift gas: n is a radical of2(ii) a IMS temperature: 45 ℃; temperature of the sample injection needle: 98 deg.C; sample introduction volume: 500 mu L of the solution; analysis time: and 15 min.
4. The method for evaluating aroma components of millets of different varieties based on gas phase ion mobility spectrometry as claimed in claim 1, wherein the step 3 collects data of retention time, migration rate and relative ion peak intensity, and establishes a fingerprint spectrum based on the data, the ordinate is gas phase retention time, the abscissa is ion migration time, the left vertical line is RIP peak (reaction ion peak, drift time is 8.03ms), and each point on two sides of the RIP peak represents the concentration of one volatile organic compound; the RIP peak is interrupted because the charges carried by the hydrated protons are taken away by the substances with the same gas phase retention time on the right side; and qualitative analysis is carried out on the substances by adopting an NIST gas phase retention index database built in GC x IMS Library Search software and an IMS migration time database of G.A.S.
5. The method for evaluating the aroma components of millets of different varieties based on gas phase ion mobility spectrometry as claimed in claim 1, wherein the step 4 utilizes a comparison method, namely extracting the characteristic areas of different millets fingerprint spectra according to the difference of peak intensity signals or colors of characteristic substances in the fingerprint spectra; the characteristic region of the millet fingerprint consists of all volatile organic matter signal peaks contained in the sample millet, and each column is an organic matter under the same retention time and drift time, namely the signal peaks of the same substances in different samples.
6. The method for evaluating the aroma components of the millets of different varieties based on the gas phase ion mobility spectrometry as claimed in claim 1, wherein the step 5 is to establish a classification model by a principal component analysis method, pre-process the data before establishing the classification model, specifically, filter the data by a standard deviation option, normalize the data by using median standardization, convert the logarithmic data, and finally analyze the principal component after full-range scale processing; the similarity between different varieties of millets can be seen through the principal component analysis result, and the differentiation of different millet samples is completed.
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CN113390980A (en) * | 2021-05-24 | 2021-09-14 | 中国农业科学院农产品加工研究所 | Method for evaluating flavor substance change in pancake processing |
CN113533551A (en) * | 2021-06-08 | 2021-10-22 | 广西科技大学 | GC-IMS-based fragrant rice shared flavor fingerprint spectrum extraction method |
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CN113390980B (en) * | 2021-05-24 | 2023-08-25 | 中国农业科学院农产品加工研究所 | Evaluation method for flavor substance change in pancake processing |
CN113533551A (en) * | 2021-06-08 | 2021-10-22 | 广西科技大学 | GC-IMS-based fragrant rice shared flavor fingerprint spectrum extraction method |
CN113533551B (en) * | 2021-06-08 | 2023-10-03 | 广西科技大学 | GC-IMS-based extraction method of fragrant rice sharing flavor fingerprint spectrum |
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